ASTM C1109-98
(Test Method)Standard Test Method for Analysis of Aqueous Leachates from Nuclear Waste Materials Using Inductively Coupled Plasma-Atomic Emission Spectrometry
Standard Test Method for Analysis of Aqueous Leachates from Nuclear Waste Materials Using Inductively Coupled Plasma-Atomic Emission Spectrometry
SCOPE
1.1 This test method is applicable to the determination of low concentration and trace elements in aqueous leachate solutions produced by the leaching of nuclear waste materials.
1.2 The nuclear waste material may be a simulated (nonradioactive) solid waste form or an actual solid radioactive waste material.
1.3 The leachate may be deionized water or any natural or simulated leachate solution containing less than 1% total dissolved solids.
1.4 The analysis must be conducted with an inductively coupled plasma-atomic emission spectrometer.
1.5 The values stated in SI units are to be regarded as the standard.
1.6 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
General Information
Relations
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: C 1109 – 98
Standard Test Method for
Analysis of Aqueous Leachates from Nuclear Waste
Materials Using Inductively Coupled Plasma-Atomic
Emission Spectroscopy
This standard is issued under the fixed designation C 1109; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope 3.1.1 deemission spectroscopy—refer to Terminology
E 135.
1.1 This test method is applicable to the determination of
3.1.2 water—refer to Terminology D 1129.
low concentration and trace elements in aqueous leachate
3.2 Definitions of Terms Specific to This Standard:
solutions produced by the leaching of nuclear waste materials.
3.2.1 analytical curve—the plot of net signal intensity
1.2 The nuclear waste material may be a simulated (nonra-
versus elemental concentration using data obtained during
dioactive) solid waste form or an actual solid radioactive waste
calibration.
material.
3.2.2 calibration—the process by which the relationship
1.3 The leachate may be deionized water or any natural or
between net signal intensity and elemental concentration is
simulated leachate solution containing less than 1 % total
determined for a specific element analysis.
dissolved solids.
3.2.3 calibration blank—a 1 % (v/v) solution of nitric acid
1.4 The analysis must be conducted with an inductively
in deionized water.
coupled plasma-atomic emission spectrometer.
3.2.4 calibration reference solution(s)—solutions contain-
1.5 The values stated in SI units are to be regarded as the
ing known concentrations of one or more elements in 1 % (v/v)
standard.
nitric acid for instrument calibration.
1.6 This standard does not purport to address all of the
3.2.5 detection limits (DL)—the concentration of the ana-
safety problems, if any, associated with its use. It is the
lyte element equivalent to three times the standard deviation of
responsibility of the user of this standard to establish appro-
ten replicate measurements of the matrix blank.
priate safety and health practices and determine the applica-
3.2.6 instrument check solution(s)—solution(s) containing
bility of regulatory limitations prior to use.
all the elements to be determined at concentration levels
2. Referenced Documents approximating the concentrations in the specimens. These
solutions must also contain 1 % (v/v) nitric acid.
2.1 ASTM Standards:
3.2.7 linear dynamic range—the elemental concentration
C 1009 Guide for Establishing a Quality Assurance Pro-
range over which the analytical curve remains linear to within
gram for Analytical Chemistry Laboratories Within the
the precision of the analytical method.
Nuclear Industry
3.2.8 linearity check solution(s)—solution(s) containing the
C 1220 Test Method for Static Leaching of Monolithic
elements to be determined at concentrations that cover a range
Waste Forms for Disposal of Radioactive Wastes
that is two to ten times higher and lower than the concentration
D 1129 Terminology Relating to Water
of these elements in the calibration reference solutions. These
D 1193 Specification for Reagent Water
solutions also contain 1 % (v/v) nitric acid.
E 135 Terminology Relating to Analytical Chemistry for
3.2.9 nonspectral interference—changes in the apparent net
Metals, Ores, and Related Materials
signal intensity from the analyte due to physical or chemical
3. Terminology
processes that affect the transport of the analyte to the plasma
and its vaporization, atomization, or excitation in the plasma.
3.1 Definitions:
3.2.10 off-peak background correction—during specimen
analysis, measurements are made of the background intensity
This test method is under the jurisdiction of ASTM Committee C-26 on Nuclear
near the peak wavelength of the analytical lines. Correction of
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
the analytical line peak intensity to yield the net line intensity
Test.
can be made by subtraction of either (a) a single intensity
Current edition approved July 10, 1998. Published October 1998. Originally
published as C 1109 – 88. Last previous edition C 1109 – 93.
measurement performed on the high or low wavelength side of
Annual Book of ASTM Standards, Vol 12.01.
the analytical line (single-point background correction), or (b)
Annual Book of ASTM Standards, Vol 11.01.
Annual Book of ASTM Standards, Vol 03.05.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
C 1109
an interpolated background intensity from background mea- spectrometer may be of the simultaneous multielement or
surements acquired on both the high and low wavelength sides sequential scanning type. The spectrometer may be of the
of the analytical line (double-point background correction). air-path, inert gas-path, or vacuum type, with spectral lines
3.2.11 on-peak spectral interference correction— selected appropriately for use with the specific instrument.
adjustments made in observed net intensity of peak of interest Either an analog or digital readout system may be used.
to compensate for error introduced by spectral interferences.
7. Reagents and Materials
3.2.12 sensitivity—the slope of the linear dynamic range.
7.1 Purity of Reagents—Reagent grade chemicals shall be
3.2.13 specific interference—light emission from spectral
used in all tests. Unless otherwise indicated, it is intended that
sources other than the analyte element that contributes to the
all reagents conform to the specifications of the Committee on
apparent net signal intensity of the analyte. Sources of spectral
Analytical Reagents of the American Chemical Society where
interference include spectral line overlaps, broadened wings of
such specifications are available. Other grades may be used,
intense spectral lines, ion-atom recombination continuum
provided it is first ascertained that the reagent is of sufficiently
emission, molecular band emission, and stray (scattered) light
high purity to permit its use without lessening the accuracy of
effects.
the determination.
4. Summary of Test Method 7.2 Purity of Water—Unless otherwise indicated, references
to water shall be understood to mean reagent water as defined
4.1 The general principles of emission spectrometric analy-
by Type I of Specification D 1193 or water exceeding these
sis are given in Ref (1). In this test method, elemental
specifications.
constituents of aqueous leachate solutions are determined
7.3 Nitric Acid (specific gravity 1.42)—Concentrated nitric
simultaneously or sequentially by inductively coupled plasma-
acid (HNO ).
atomic emission spectroscopy (ICP-AES). 3
7.4 Nitric Acid, High-Purity—Nitric acid of higher purity
4.2 Specimens are prepared by filtration if needed to remove
than reagent grade, specially prepared to be low in metallic
particulates and acidification to match calibration reference
contaminants. The acid may be prepared by sub-boiling distil-
solutions. Filtration should be the last resort to clarify a
lation (2), or purchased from commercial sources.
solution since leach studies are designed to determine the
7.5 Stock Solutions—May be purchased or prepared from
absolutre amount of glass dissolved.
metals or metal salts of known purity. Stock solutions should
4.3 Additional general guidelines are provided in Guide
contain known concentrations of the element of interest rang-
C 1009, Terminology D 1129, Specification D 1193, and Ter-
ing from 100 to 10 000 mg/L.
minology E 135.
7.6 Calibration Reference Solutions, Instrument Check So-
5. Significance and Use lutions, and Linearity Check Solutions:
7.6.1 Prepare single-element or multielement calibration
5.1 This test method may be used to determine concentra-
reference solutions by combining appropriate volumes of the
tions of elements leached from nuclear waste materials
stock solutions in acid-rinsed volumetric flasks. To establish
(glasses, ceramics, cements) using an aqueous leachant. If the
the calibration slope accurately, provide at least one solution
nuclear waste material is radioactive, a suitably contained and
with element concentration that is a minimum of 100 times the
shielded ICP-AES spectrometer system with a filtered exit-gas
detection limit for each element. Add sufficient nitric acid to
system must be used, but no other changes in the test method
bring the final solution to 1 % HNO . Prior to preparing the
are required. The leachant may be deionized water or any
multielement solutions, analyze each stock solution separately
aqueous solution containing less than 1 % total solids.
to check for strong spectral interference and the presence of
5.2 This test method as written is for the analysis of
impurities (3). Take care when preparing the multielement
solutions containing 1 % (v/v) nitric acid. It can be modified to
solutions to verify that the components are compatible and
specify the use of the same or another mineral acid at the same
stable (they do not interact to cause precipitation) and that none
or higher concentration. In such cases, the only change needed
of the elements present exhibit mutual spectral interference.
in this test method is to substitute the preferred acid and
Transfer the calibration reference solutions to acid-leached
concentration value whenever 1 % nitric acid appears here. It is
FEP TFE-fluorocarbon or polyethylene bottles for storage.
important that the acid type and content of the reference and
Calibration reference solutions must be verified initially using
check solutions closely match the leachate solutions to be
a quality control sample and monitored periodically for stabil-
analyzed.
ity.
5.3 This test method can be used to analyze leachates from
static leach testing of waste forms using C 1220.
NOTE 1—Solutions in polyethylene bottles are subject to transpiration
losses that may affect the assigned concentration values.
6. Apparatus
7.6.2 Prepare the instrument check solution(s) and linearity
6.1 Inductively Coupled Plasma-Atomic Emission Spec-
check solutions in a similar manner.
trometer, with a spectral bandpass of 0.05 nm or less, is
required to provide the necessary spectral resolution. The
“Reagent Chemicals, American Chemical Society Specifications,” Am. Chem-
ical Soc., Washington DC. For suggestions on the testing of reagents not listed by
the American Chemical Society, see “Reagent Chemicals and Standards,” by Joseph
The boldface numbers in parentheses refer to the list of references at the end Rosin, D. Van Nostrand Co., Inc., New York, NY, and the “United States
of this standard. Pharmacopeia.”
C 1109
TABLE 1 1Suggested Analytical Wavelengths of Typical
7.6.3 Fresh solutions should be prepared as needed with the
A
Elements for ICP-AES
realization that concentrations can change with age.
Suggested Estimated Alternative Estimated
Element Wavelength, Detection Wavelength, Detection
8. Specimen Preparation
nm Limit, mg/L nm Limit, mg/L
8.1 Filter the leachate through a clean, inert membrane filter
Aluminum 308.22 0.04 237.32 0.03
Americium 283.23 0.01 292.06 >0.01
having pore size of 0.45 μm or smaller, using an inert filter
B
Arsenic 193.70 0.05 189.04 0.01
support (avoid the use of fritted glass supports). Examine the
Barium 493.41 0.002 455.40 0.001
filtered leachate to verify the absence of visible solids or
Beryllium 234.86 0.0003 313.04 0.0003
Boron 249.77 0.005 249.68 0.005
suspended colloids. Compare the analyses of filtered and
Cadmium 214.44 0.002 . .
unfiltered aliquots of the original leachate solution to determine
Calcium 317.93 0.01 393.37 0.0002
whether the filter membrane contributes to the blank level of
Cerium 418.66 0.05 413.76 0.05
Chromium 267.72 0.007 205.55 0.006
the filtered solution. The deposit on the filter may be analyzed
Dysprosium 353.17 0.01 205.50 .
separately if required.
Gadolinium 342.25 0.01 . .
8.2 Add sufficient high-purity concentrated nitric acid to
Iron 259.94 0.006 273.96 0.02
Lanthanum 408.67 0.01 379.48 0.01
bring the leachate sample solution to volume1%HNO .Ifthe
Lead 217.00 0.09 220.35 0.04
leachate is known to be a chloride solution, or nitric acid is
Lithium 670.78 0.002 . .
undesirable for other experimental reasons, concentrated hy- Magnesium 279.55 0.0001 279.08 0.03
Manganese 257.61 0.001 294.92 0.008
drochloric or other mineral acid may be used instead. The acid
Molybdenum 202.03 0.008 203.84 0.01
conditions of the calibration and check solutions used in the
Neodymium 406.11 0.1 401.22 0.05
analytical procedure must match those of the leachate speci-
Neptunium 382.91 0.09 456.04 0.13
Nickel 231.60 0.02 221.65 0.01
men.
B
Phosphorus 214.91 0.08 178.29
Plutonium 300.06 0.03 297.25 0.03
9. Analytical Conditions Potassium 766.49 0.04 . .
Rhodium 343.49 0.06 233.48 0.04
9.1 Analytical Lines—Suggested analytical lines for typical
Ruthenium 240.27 0.03 . .
Samarium 442.43 0.05 . .
elements are given in Table 1. Additional lines for these and
B
Selenium 203.99 0.1 196.03 0.08
other elements of interest, and information about possible
Silicon 288.16 0.03 212.41 0.02
interfering lines, can be found in compilations of analytical
Sodium 589.00 0.03 330.24 1.9
Strontium 421.55 0.0008 407.77 0.0004
lines for ICP-AES (4-12).
B
Sulfur 180.73 . .
9.2 Selection of Analytical Conditions—Select an optimum
Technetium 254.32 0.002 261.00 0.002
combination of analytical lines, background correction meth-
Tellurium 214.28 0.04 214.72 0.2
Thorium 401.91 0.08 . .
ods, plasma viewing position, and plasma/spectrometer oper-
Titanium 337.28 0.007 334.94 0.004
ating conditions to obtain the following for each element:
Uranium 385.96 0.25 367.01 0.3
9.2.1 The lowest attainable detection limit,
Vanadium 292.40 0.008 . .
Zinc 213.86 0.002 206.20 0.006
9.2.2 The acceptable linear dynamic range,
Zirconium 343.82 0.008 339.20 0.008
9.2.3 Avoidance or minimization of spectral and nonspectral
A
See Refs (4-12) for a more complete list. Check those references also to
interference, and
identify any possible interfering spectral lines from components such as rare
9.2.4 Best attainable precision. earths, actinides, or high-concentration components.
B
Vacuum spectrometer.
9.3 Follow the spectrometer manufacturer’s recommenda-
tion wherever possible in establishing operating conditions.
For simultaneous multielement systems, the optimum plasma
10. Calibration
viewing position and set of operating conditions is usually a
compromise (13). The combination of conditions selected must 10.1 Calibration of the Spectrometer System:
be used
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.